# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1318 # CIF belonging to Paper -2-Hydroxy-benzylidene .. - Ligtenbarg et al. # CIF-file generated for s1720a #============================================================================== data_global #============================================================================== # 0. AUDIT DETAILS _audit_creation_date 'Wed Sep 23 15:53:22 1998' _audit_creation_method 'PLATON option' #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondence ; Dr. A.L. Spek ; _publ_contact_author_address # Address of author for correspondence ; Bijvoet Center for Biomolecular Research Department of Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; _publ_contact_author_email 'spea@chem.uu.nl' _publ_contact_author_fax '+31 30 2533940' _publ_contact_author_phone '+31 30 2532538' #=============================================================================== data_s1720a #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_moiety 'C18 H12 N3 O3 V' _chemical_formula_sum 'C18 H12 N3 O3 V' _chemical_formula_weight 369.25 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 7.0787(16) _cell_length_b 16.833(5) _cell_length_c 13.573(5) _cell_angle_alpha 90 _cell_angle_beta 115.21(2) _cell_angle_gamma 90 _cell_volume 1463.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 0.70 _exptl_absorpt_correction_type delref _exptl_absorpt_process_details PLATON/DELABS _exptl_absorpt_correction_T_min 0.143 _exptl_absorpt_correction_T_max 0.615 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4T' _diffrn_measurement_method 'omega-scan' # number of measured reflections (redundant set) _diffrn_reflns_number 6346 _diffrn_reflns_av_R_equivalents 0.1061 _diffrn_reflns_av_sigmaI/netI 0.1155 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 26.50 # number of unique reflections _reflns_number_total 3006 # number of observed reflections (> n sig(I)) _reflns_number_gt 1984 _reflns_threshold_expression 'I>2sigma(i)' _computing_data_collection 'Locally modified CAD4-Version 5 Software' _computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)' _computing_data_reduction 'HELENA (Spek, 1997)' _computing_structure_solution 'SHELXS86' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment 'H-atom refinement: see text ' _refine_ls_extinction_method none _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack none _refine_ls_number_reflns 3006 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0992 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1415 _refine_ls_wR_factor_gt 0.1237 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.592 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.089 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv V1 V Uani 0.48998(12) 0.57903(4) 0.30698(5) 1.000 0.0219(2) O1 O Uani 0.3133(5) 0.52189(16) 0.1818(2) 1.000 0.0253(8) O2 O Uani 0.6349(5) 0.63471(18) 0.2711(2) 1.000 0.0279(9) O3 O Uani 0.3167(5) 0.63423(16) 0.3241(2) 1.000 0.0262(9) N1 N Uani 0.6258(5) 0.46685(18) 0.3526(2) 1.000 0.0198(9) N2 N Uani 0.7201(5) 0.34208(18) 0.3607(2) 1.000 0.0184(9) N3 N Uani 0.6724(6) 0.58101(19) 0.4825(2) 1.000 0.0238(10) C1 C Uani 0.3605(7) 0.4666(2) 0.1253(3) 1.000 0.0217(11) C2 C Uani 0.2540(7) 0.4697(3) 0.0107(3) 1.000 0.0272(12) C3 C Uani 0.2977(7) 0.4159(3) -0.0526(3) 1.000 0.0290(11) C4 C Uani 0.4446(7) 0.3575(2) -0.0060(3) 1.000 0.0274(14) C5 C Uani 0.5466(7) 0.3516(2) 0.1063(3) 1.000 0.0254(12) C6 C Uani 0.5034(7) 0.4043(2) 0.1738(3) 1.000 0.0206(11) C7 C Uani 0.6107(6) 0.4031(2) 0.2921(3) 1.000 0.0207(11) C8 C Uani 0.7459(6) 0.4491(2) 0.4597(3) 1.000 0.0194(11) C9 C Uani 0.8104(6) 0.3712(2) 0.4686(3) 1.000 0.0191(11) C10 C Uani 0.9354(7) 0.3194(2) 0.5528(3) 1.000 0.0228(11) C11 C Uani 0.9658(7) 0.2433(2) 0.5288(3) 1.000 0.0287(14) C12 C Uani 0.8611(7) 0.2148(2) 0.4192(3) 1.000 0.0276(14) C13 C Uani 0.7407(7) 0.2624(2) 0.3392(3) 1.000 0.0249(14) C14 C Uani 0.7792(6) 0.5152(2) 0.5338(3) 1.000 0.0195(11) C15 C Uani 0.9054(7) 0.5146(2) 0.6466(3) 1.000 0.0237(11) C16 C Uani 0.9135(7) 0.5836(3) 0.7038(3) 1.000 0.0282(14) C17 C Uani 0.8032(7) 0.6500(3) 0.6519(3) 1.000 0.0298(14) C18 C Uani 0.6830(7) 0.6464(2) 0.5402(3) 1.000 0.0275(14) H2 H Uiso 0.15110 0.50940 -0.02290 1.000 0.0330 H3 H Uiso 0.22550 0.41910 -0.12960 1.000 0.0350 H4 H Uiso 0.47600 0.32130 -0.05070 1.000 0.0320 H5 H Uiso 0.64780 0.31100 0.13820 1.000 0.0300 H10 H Uiso 0.99820 0.33760 0.62610 1.000 0.0270 H11 H Uiso 1.05630 0.20910 0.58470 1.000 0.0340 H12 H Uiso 0.87820 0.16090 0.40360 1.000 0.0330 H13 H Uiso 0.66860 0.24230 0.26740 1.000 0.0300 H15 H Uiso 0.98220 0.46870 0.68220 1.000 0.0280 H16 H Uiso 0.99670 0.58500 0.78020 1.000 0.0340 H17 H Uiso 0.80910 0.69720 0.69140 1.000 0.0360 H18 H Uiso 0.60570 0.69200 0.50360 1.000 0.0330 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0234(4) 0.0206(3) 0.0224(3) 0.0031(3) 0.0105(3) 0.0018(3) O1 0.0252(16) 0.0258(14) 0.0239(14) 0.0003(11) 0.0095(13) 0.0042(14) O2 0.0260(17) 0.0359(16) 0.0228(14) 0.0020(12) 0.0113(13) -0.0010(15) O3 0.0290(18) 0.0240(14) 0.0288(14) 0.0026(12) 0.0153(14) 0.0049(14) N1 0.0208(19) 0.0181(15) 0.0184(15) 0.0013(13) 0.0063(14) 0.0018(15) N2 0.0175(18) 0.0179(15) 0.0205(16) 0.0001(13) 0.0088(15) 0.0010(14) N3 0.026(2) 0.0232(16) 0.0237(16) -0.0029(14) 0.0119(15) -0.0024(17) C1 0.027(2) 0.0208(19) 0.0221(19) -0.0015(15) 0.0151(18) -0.0028(18) C2 0.024(2) 0.030(2) 0.026(2) 0.0090(17) 0.0092(19) 0.002(2) C3 0.030(2) 0.034(2) 0.0209(19) -0.0003(18) 0.0089(19) -0.006(2) C4 0.031(3) 0.029(2) 0.0203(19) -0.0043(17) 0.0092(19) -0.005(2) C5 0.026(2) 0.023(2) 0.026(2) 0.0007(16) 0.0099(19) 0.0008(19) C6 0.022(2) 0.0214(19) 0.0181(18) -0.0007(14) 0.0082(17) -0.0029(18) C7 0.020(2) 0.023(2) 0.0201(18) -0.0005(15) 0.0095(18) 0.0002(17) C8 0.017(2) 0.0224(18) 0.0179(18) 0.0020(15) 0.0066(16) -0.0016(17) C9 0.014(2) 0.0242(19) 0.0163(18) 0.0004(15) 0.0037(16) -0.0025(17) C10 0.019(2) 0.030(2) 0.0190(19) 0.0034(16) 0.0078(17) -0.0007(19) C11 0.026(3) 0.027(2) 0.031(2) 0.0085(18) 0.010(2) 0.003(2) C12 0.030(3) 0.0213(19) 0.034(2) 0.0004(17) 0.016(2) 0.000(2) C13 0.029(3) 0.0184(19) 0.027(2) -0.0059(16) 0.0116(19) -0.0033(19) C14 0.015(2) 0.0217(19) 0.0237(19) 0.0003(15) 0.0102(17) -0.0001(17) C15 0.025(2) 0.029(2) 0.0182(19) 0.0030(16) 0.0102(18) -0.0045(19) C16 0.029(3) 0.036(2) 0.024(2) -0.0040(19) 0.0154(19) -0.011(2) C17 0.037(3) 0.025(2) 0.037(2) -0.0092(18) 0.025(2) -0.008(2) C18 0.029(3) 0.024(2) 0.030(2) 0.0007(17) 0.013(2) 0.002(2) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O1 1.888(3) . . yes V1 O2 1.610(4) . . yes V1 O3 1.632(4) . . yes V1 N1 2.090(3) . . yes V1 N3 2.173(3) . . yes O1 C1 1.336(5) . . yes N1 C7 1.328(5) . . yes N1 C8 1.368(5) . . yes N2 C7 1.381(5) . . yes N2 C9 1.413(4) . . yes N2 C13 1.393(5) . . yes N3 C14 1.355(5) . . yes N3 C18 1.334(5) . . yes C1 C2 1.411(5) . . no C1 C6 1.410(6) . . no C2 C3 1.371(7) . . no C3 C4 1.374(6) . . no C4 C5 1.385(5) . . no C5 C6 1.399(6) . . no C6 C7 1.455(5) . . no C8 C9 1.377(5) . . no C8 C14 1.450(5) . . no C9 C10 1.410(5) . . no C10 C11 1.361(5) . . no C11 C12 1.433(5) . . no C12 C13 1.326(5) . . no C14 C15 1.406(5) . . no C15 C16 1.385(6) . . no C16 C17 1.374(7) . . no C17 C18 1.388(5) . . no C2 H2 0.9498 . . no C3 H3 0.9494 . . no C4 H4 0.9506 . . no C5 H5 0.9505 . . no C10 H10 0.9511 . . no C11 H11 0.9505 . . no C12 H12 0.9511 . . no C13 H13 0.9492 . . no C15 H15 0.9499 . . no C16 H16 0.9500 . . no C17 H17 0.9494 . . no C18 H18 0.9507 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 V1 O2 106.70(14) . . . yes O1 V1 O3 99.68(15) . . . yes O1 V1 N1 81.44(12) . . . yes O1 V1 N3 148.28(13) . . . yes O2 V1 O3 109.02(16) . . . yes O2 V1 N1 110.10(16) . . . yes O2 V1 N3 99.50(15) . . . yes O3 V1 N1 138.68(15) . . . yes O3 V1 N3 88.10(14) . . . yes N1 V1 N3 72.87(12) . . . yes V1 O1 C1 129.8(3) . . . yes V1 N1 C7 129.9(2) . . . yes V1 N1 C8 120.8(2) . . . yes C7 N1 C8 109.3(3) . . . yes C7 N2 C9 108.5(3) . . . yes C7 N2 C13 130.8(3) . . . yes C9 N2 C13 120.6(3) . . . yes V1 N3 C14 119.5(2) . . . yes V1 N3 C18 121.0(3) . . . yes C14 N3 C18 119.6(3) . . . yes O1 C1 C2 117.4(4) . . . yes O1 C1 C6 123.7(3) . . . yes C2 C1 C6 118.8(4) . . . no C1 C2 C3 120.6(4) . . . no C2 C3 C4 120.8(4) . . . no C3 C4 C5 119.7(4) . . . no C4 C5 C6 121.2(4) . . . no C1 C6 C5 118.6(3) . . . no C1 C6 C7 117.3(3) . . . no C5 C6 C7 123.8(4) . . . no N1 C7 N2 108.0(3) . . . yes N1 C7 C6 122.6(3) . . . yes N2 C7 C6 129.3(3) . . . yes N1 C8 C9 109.5(3) . . . yes N1 C8 C14 114.4(3) . . . yes C9 C8 C14 136.1(4) . . . no N2 C9 C8 104.6(3) . . . yes N2 C9 C10 118.4(3) . . . yes C8 C9 C10 136.9(3) . . . no C9 C10 C11 119.8(3) . . . no C10 C11 C12 119.9(3) . . . no C11 C12 C13 121.0(3) . . . no N2 C13 C12 119.9(3) . . . yes N3 C14 C8 112.4(3) . . . yes N3 C14 C15 121.5(3) . . . yes C8 C14 C15 126.1(3) . . . no C14 C15 C16 117.4(3) . . . no C15 C16 C17 121.1(4) . . . no C16 C17 C18 118.3(4) . . . no N3 C18 C17 122.1(4) . . . yes C1 C2 H2 119.71 . . . no C3 C2 H2 119.69 . . . no C2 C3 H3 119.53 . . . no C4 C3 H3 119.63 . . . no C3 C4 H4 120.11 . . . no C5 C4 H4 120.17 . . . no C4 C5 H5 119.44 . . . no C6 C5 H5 119.34 . . . no C9 C10 H10 120.07 . . . no C11 C10 H10 120.16 . . . no C10 C11 H11 120.03 . . . no C12 C11 H11 120.04 . . . no C11 C12 H12 119.47 . . . no C13 C12 H12 119.50 . . . no N2 C13 H13 119.98 . . . no C12 C13 H13 120.15 . . . no C14 C15 H15 121.35 . . . no C16 C15 H15 121.27 . . . no C15 C16 H16 119.42 . . . no C17 C16 H16 119.49 . . . no C16 C17 H17 120.84 . . . no C18 C17 H17 120.82 . . . no N3 C18 H18 118.91 . . . no C17 C18 H18 118.95 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 V1 O1 C1 66.0(3) . . . . no O3 V1 O1 C1 179.4(3) . . . . no N1 V1 O1 C1 -42.5(3) . . . . no N3 V1 O1 C1 -78.4(5) . . . . no O1 V1 N1 C7 18.2(4) . . . . no O1 V1 N1 C8 -159.2(3) . . . . no O2 V1 N1 C7 -86.6(4) . . . . no O2 V1 N1 C8 96.1(3) . . . . no O3 V1 N1 C7 113.1(4) . . . . no O3 V1 N1 C8 -64.3(4) . . . . no N3 V1 N1 C7 179.4(4) . . . . no N3 V1 N1 C8 2.0(3) . . . . no O1 V1 N3 C14 37.8(5) . . . . no O1 V1 N3 C18 -143.1(4) . . . . no O2 V1 N3 C14 -107.8(4) . . . . no O2 V1 N3 C18 71.3(4) . . . . no O3 V1 N3 C14 143.3(4) . . . . no O3 V1 N3 C18 -37.7(4) . . . . no N1 V1 N3 C14 0.5(3) . . . . no N1 V1 N3 C18 179.5(4) . . . . no V1 O1 C1 C2 -139.2(4) . . . . no V1 O1 C1 C6 43.4(6) . . . . no V1 N1 C7 N2 -176.7(3) . . . . no V1 N1 C7 C6 6.2(7) . . . . no C8 N1 C7 N2 0.9(5) . . . . no C8 N1 C7 C6 -176.2(4) . . . . no V1 N1 C8 C9 177.8(3) . . . . no V1 N1 C8 C14 -4.0(5) . . . . no C7 N1 C8 C9 0.0(5) . . . . no C7 N1 C8 C14 178.2(4) . . . . no C9 N2 C7 N1 -1.4(5) . . . . no C9 N2 C7 C6 175.4(5) . . . . no C13 N2 C7 N1 175.0(4) . . . . no C13 N2 C7 C6 -8.2(8) . . . . no C7 N2 C9 C8 1.3(5) . . . . no C7 N2 C9 C10 -178.2(4) . . . . no C13 N2 C9 C8 -175.5(4) . . . . no C13 N2 C9 C10 5.0(6) . . . . no C7 N2 C13 C12 178.0(5) . . . . no C9 N2 C13 C12 -5.9(7) . . . . no V1 N3 C14 C8 -2.5(5) . . . . no V1 N3 C14 C15 177.6(3) . . . . no C18 N3 C14 C8 178.4(4) . . . . no C18 N3 C14 C15 -1.5(7) . . . . no V1 N3 C18 C17 -178.1(4) . . . . no C14 N3 C18 C17 1.0(7) . . . . no O1 C1 C2 C3 178.6(5) . . . . no C6 C1 C2 C3 -3.8(7) . . . . no C2 C1 C6 C7 179.9(3) . . . . no C2 C1 C6 C5 5.1(7) . . . . no O1 C1 C6 C5 -177.5(4) . . . . no O1 C1 C6 C7 -2.7(7) . . . . no C1 C2 C3 C4 0.5(8) . . . . no C2 C3 C4 C5 1.5(7) . . . . no C3 C4 C5 C6 -0.2(7) . . . . no C4 C5 C6 C1 -3.1(7) . . . . no C4 C5 C6 C7 -177.6(4) . . . . no C1 C6 C7 N1 -19.4(7) . . . . no C1 C6 C7 N2 164.3(4) . . . . no C5 C6 C7 N1 155.1(4) . . . . no C5 C6 C7 N2 -21.2(8) . . . . no N1 C8 C9 C10 178.6(5) . . . . no C14 C8 C9 N2 -178.5(5) . . . . no N1 C8 C9 N2 -0.8(5) . . . . no C9 C8 C14 C15 1.4(9) . . . . no C14 C8 C9 C10 0.9(10) . . . . no N1 C8 C14 N3 4.0(6) . . . . no N1 C8 C14 C15 -176.2(4) . . . . no C9 C8 C14 N3 -178.4(5) . . . . no C8 C9 C10 C11 -179.5(5) . . . . no N2 C9 C10 C11 -0.2(7) . . . . no C9 C10 C11 C12 -3.6(7) . . . . no C10 C11 C12 C13 2.8(8) . . . . no C11 C12 C13 N2 2.1(8) . . . . no N3 C14 C15 C16 1.1(7) . . . . no C8 C14 C15 C16 -178.7(5) . . . . no C14 C15 C16 C17 -0.4(8) . . . . no C15 C16 C17 C18 -0.1(8) . . . . no C16 C17 C18 N3 -0.2(8) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag V1 C12 3.785(4) . 2_655 no V1 C13 3.657(4) . 2_655 no V1 C15 3.495(5) . 3_666 no V1 C16 3.914(5) . 3_666 no V1 C14 3.785(4) . 3_666 no V1 H12 3.2427 . 2_655 no V1 H13 2.9778 . 2_655 no V1 H15 3.5010 . 3_666 no O1 C15 3.357(6) . 3_666 no O1 C16 3.204(6) . 3_666 no O2 C10 3.061(6) . 3_766 no O2 C13 3.246(5) . 2_655 no O2 C3 3.310(5) . 3_665 no O2 C4 3.399(5) . 3_665 no O3 C15 3.072(5) . 3_666 no O3 C10 3.021(6) . 3_666 no O3 C14 3.409(5) . 3_666 no O3 C9 3.300(5) . 3_666 no O3 C13 2.994(5) . 2_655 no O3 C12 3.285(5) . 2_655 no O1 H12 2.7052 . 2_655 no O2 H3 2.6650 . 3_665 no O2 H10 2.4130 . 3_766 no O2 H4 2.8483 . 3_665 no O2 H13 2.6856 . 2_655 no O3 H13 2.2299 . 2_655 no O3 H12 2.8327 . 2_655 no O3 H18 2.6116 . . no O3 H10 2.6333 . 3_666 no O3 H15 2.7077 . 3_666 no N1 C15 3.329(7) . 3_766 no N2 C16 3.316(6) . 3_766 no N3 C10 3.447(6) . 3_766 no N3 C8 3.409(6) . 3_666 no N2 H5 2.8878 . . no C1 C3 3.574(7) . 3_665 no C2 C3 3.545(7) . 3_665 no C3 C2 3.545(7) . 3_665 no C3 O2 3.310(5) . 3_665 no C3 C1 3.574(7) . 3_665 no C4 O2 3.399(5) . 3_665 no C5 C13 3.230(5) . . no C7 C15 3.452(7) . 3_766 no C7 C16 3.352(7) . 3_766 no C7 C17 3.444(7) . 3_666 no C8 N3 3.409(6) . 3_666 no C8 C15 3.403(7) . 3_766 no C8 C14 3.379(7) . 3_766 no C8 C18 3.436(7) . 3_666 no C9 C18 3.456(7) . 3_666 no C9 C14 3.490(6) . 3_766 no C9 O3 3.300(5) . 3_666 no C9 C15 3.587(6) . 3_766 no C10 O3 3.021(6) . 3_666 no C10 O2 3.061(6) . 3_766 no C10 C15 3.563(5) . . no C10 C18 3.482(7) . 3_766 no C10 N3 3.447(6) . 3_766 no C11 C18 3.534(7) . 3_766 no C12 O3 3.285(5) . 2_645 no C12 V1 3.785(4) . 2_645 no C13 C5 3.230(5) . . no C13 O2 3.246(5) . 2_645 no C13 C17 3.504(7) . 3_766 no C13 O3 2.994(5) . 2_645 no C13 V1 3.657(4) . 2_645 no C14 C8 3.379(7) . 3_766 no C14 V1 3.785(4) . 3_666 no C14 O3 3.409(5) . 3_666 no C14 C9 3.490(6) . 3_766 no C15 C7 3.452(7) . 3_766 no C15 O1 3.357(6) . 3_666 no C15 O3 3.072(5) . 3_666 no C15 C9 3.587(6) . 3_766 no C15 N1 3.329(7) . 3_766 no C15 V1 3.495(5) . 3_666 no C15 C8 3.403(7) . 3_766 no C15 C10 3.563(5) . . no C16 N2 3.316(6) . 3_766 no C16 O1 3.204(6) . 3_666 no C16 C7 3.352(7) . 3_766 no C16 V1 3.914(5) . 3_666 no C17 C7 3.444(7) . 3_666 no C17 C13 3.504(7) . 3_766 no C18 C9 3.456(7) . 3_666 no C18 C8 3.436(7) . 3_666 no C18 C11 3.534(7) . 3_766 no C18 C10 3.482(7) . 3_766 no C2 H2 2.9629 . 3_565 no C3 H12 3.0560 . 4_454 no C4 H18 2.8105 . 2_645 no C5 H18 3.0389 . 2_645 no C5 H13 2.7025 . . no C6 H13 3.0253 . . no C9 H15 3.0942 . . no C10 H15 3.0025 . . no C12 H4 2.9860 . 4_555 no C13 H5 2.6488 . . no C15 H10 3.0890 . . no H2 C2 2.9629 . 3_565 no H2 H2 2.4891 . 3_565 no H3 H15 2.5378 . 1_454 no H3 O2 2.6650 . 3_665 no H4 H18 2.4073 . 2_645 no H4 O2 2.8483 . 3_665 no H4 C12 2.9860 . 4_554 no H5 N2 2.8878 . . no H5 C13 2.6488 . . no H5 H13 2.0529 . . no H10 C15 3.0890 . . no H10 H15 2.3529 . . no H10 O2 2.4130 . 3_766 no H10 O3 2.6333 . 3_666 no H12 V1 3.2427 . 2_645 no H12 O1 2.7052 . 2_645 no H12 O3 2.8327 . 2_645 no H12 C3 3.0560 . 4_655 no H13 C5 2.7025 . . no H13 C6 3.0253 . . no H13 H5 2.0529 . . no H13 V1 2.9778 . 2_645 no H13 O2 2.6856 . 2_645 no H13 O3 2.2299 . 2_645 no H15 C9 3.0942 . . no H15 C10 3.0025 . . no H15 H3 2.5378 . 1_656 no H15 H10 2.3529 . . no H15 V1 3.5010 . 3_666 no H15 O3 2.7077 . 3_666 no H18 O3 2.6116 . . no H18 C4 2.8105 . 2_655 no H18 C5 3.0389 . 2_655 no H18 H4 2.4073 . 2_655 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C10 H10 O2 0.9511 2.4130 3.061(6) 125.14 3_766 yes C13 H13 O3 0.9492 2.2299 2.994(5) 136.92 2_645 yes # End of Crystallographic Information File #=========================================================================== # Dr. A.L.Spek, Laboratory of Crystal and Structural Chemistry # # Bijvoet Center for Biomolecular Research, Utrecht University. # # (Kruytgebouw, room N801), Padualaan 8, 3584 CH Utrecht, The Netherlands. # # E-mail: a.l.spek@chem.uu.nl http://www.cryst.chem.uu.nl/ # # http://www.cryst.chem.uu.nl/platon/ # # anonymous ftp: xraysoft.chem.uu.nl # # FAX : (31)-30-2533940 PHONE : (31)-30-2532538/2533/3902/3502 # #===========================================================================